Connection between chromatographic column and valve system



INVENTOR. CHARLES FERHIN BY dfl, L441 ATTORNEY C. R. FERRIN Aug. 3, 1965CONNECTION BETWEEN CHROMATOGRAPHIC COLUMN AND VALVE SYSTEM Filed March27, 1963 FROM VALVE SYSTEM gin-i 3,198,001 CONNECTION BETWEENCHROMATGGRAPHIC COLUMN AND VALVE SYSTEM Charles R. Ferrin, Tulsa, Okla,assigns: to Instruments,

Inc., Tulsa, Okla, a corporation of Oklahoma Filed Mar. 27, 1963, Ser.No. 268,389 2 Claims. (Cl.73-23.1)

The present invention relates to connecting a chromatographic columnwith sample valves which are located in the controlled temperature of anoven.

Valve systems are used from which samples feed to a chromatographiccolumn which have their temperature controlled in order to properlyprepare the sample for introduction into the column. Also, electricalpower has been used to heat the columns for their operation. Inproviding this connection between Valves and column, there are at leastthe problems of providing .a connection which is iluid tight, providingan electrical power connection for resistance-heating of the column andmaintaining thermal stability for the sample .as the sample istransferred from the valve system 'to the column.

An object of the present invention is to provide thermal stability for asample as the sample is transferred from a valve system to achromatographic column, providing the sample without loss and providingconnection to a source of electrical power.

The present invention contemplates a controlled oven having mountedtherein a valve system for preparing a sample for insertion in achromatographic column. The body of thermal insulation is mountedadjacent the o e and a metallic union mounted on the body with a centralpassage therethrough. A conduit is mechanically communicated with theunion passage through the body of insulation and the conduit then led tothe inside of the oven. A tube for transport of the sample from thevalve system to the column extends through the conduit to communicatewith the union.

The invention further contemplates leads for electrical power extendingthrough the body of thermal insulation to the union and electricallyisolated from the valve system.

Other objects, advantages and features of this invention will becomeapparent to one skilled in the art upon consideration of the writtenspecification, appended claims, and attached drawings, wherein;

The drawing illustrates a sectioned elevation of a connection structureembodying the present invention to extend from an oven-heated valvesystem to a chromatographic column.

The drawing illustrates an oven structure 10, but the drawing does notshown the valve system mounted within the oven so the temperature of thesystem and the sample handled by the system will have its temperaturecontrolled. The source of heat for the oven, controls for the source,etc., are not shown. The structure that is shown is -a portion of oven10, provided with a lid 11 which is hinged at 12 to gain access to theinside of the oven.

A wall 13 of the oven is also partially shown, and on the outside of theoven wall a body 14 for thermal insulation is indicated. The connectionembodying the present invention is mounted within the thermal insulationbody 14.

An opening 15 is provided through wall 13 for communication between theinterior of oven and the insulation body 14. A metallic cover plate 16is provided for insulation body 14 and an access opening 17 providedthrough this plate. The connection of the present invention extendsbetween openings and 17.

The body of a union 18 of selected size is mounted over access opening17 in plate 16. In turn, the body of the union is provided with acentral passage which ex- 3,198,901 Patented Aug. 3, 1965 tendscompletely through the body. On the external side of union body 18 thecentral passage is threaded at 19 to receive tube coupling 20.

A chromatographic column 21 is .sealed into coupling 20. The junctionbetween column 21 and coupling 20 is both fluid tight and electricallycompleted.

The other, inner, end of the central passage of union 18 receives oneend of a relatively small sample tubing 22. Tube 22 is extended up intocoupling 20 for communication with column 21. Tube 22 also extends downthrough the insulation body 14, through opening 15 in wall 13 and intofluid communication with the valve system which is not shown.

Tubing 22 brings the sample to be analyzed from the valve system in oven10 to column 21. Tubing 22 is relatively long, extending from theinterior of oven 10 to junction with column 21 in coupling 20. One ofthe objects of the present invention is is to maintain the thermalstability of the sample within tubing 22. To maintain thermal stability,a comparatively large conduit 23 is provided to sheathe the tubing 22,extending from union 18 through opening 15 in wall 13.

Conduit 23 is mechanically sealed to wall opening 15 by means ofcoupling structure 24, carried in the opening 15 of wall 13. Conduit 23is, therefore, extended from coupling 24 .to union 18. This conduit 23does not touch sample tubing 22, but provides ample volume about tub ing22 for circulation of oven heat. The oven heat, conducted oversubstantially the complete length of tubing 22, maintains the tubing 22thermally stable.

A junction station is provided bet-ween the oven-end of sample tubing 22and the valve system. Junction station 25 includes a special filledTeflon body 26 which is mounted on wall :13. Tube 22 is coupled tointernal passage 27 of body 26. Station 25 provides fluid communicationbetween tube 28, coming directly from the heated valve system, andsample tube 22. At the same time, body 25 maintains the two tubeselectrically insulated from each other. Electrical power applied todirectly heat column 21 will then not be shorted through the tube 28.

A source of electrical power is provided to heat column 21. This sourceof electrical power is not shown, however, lead 29 from the source isshown, extending through insulating body 14 to complete electricalconnection with union 25) at 30. Through lead 29, the source ofelectrical power supplies the resistance-heating of column 21 while thethermally stable samples are fed to the column through tube 22.

From the foregoing it will be seen that this invention is one welladapted to attain all of the ends and objects hereinabove set forth,together with other advantages which are obvious and which are inherentto the apparatus.

It will be understood that certain features and subcombinations are ofutility and may be employed without reference to other features andsubcombinations. This is contemplated by and is within the scope of theclaims.

As many possible embodiments may be made of the invention withoutdeparting from the scope thereof, it is to be understood that all matterherein set forth or shown in the accompanying drawings is to beinterpreted as illustrative and not in a limiting sense.

The present invention having been described, what is claimed is:

1. A connection between the inlet valve system and column of a gaschromatograph, including,

an oven having a controlled intern-a1 temperature,

a thermal insulation body adjacent the oven,

a metallic union mounted on the thermal insulation body and having anaccess opening therethrough in from external the insulation body tointernal the insulation body,

a chromatograph column mechanically communicated with the external endof the access opening of the union,-

, a conduit mechanically communicated with the internal end of the unionand extending through the insulation body and into communication withthe adjacent oven,

a first tube communicated with the column through the union and extendedthrough the conduit and into the oven, a second tube fluid communicatedbetween the first tube and valve system and electrically insulated fromthe first tube,

and an electrical power lead extended through the body of insulation andinto electrical connection with the union for resistance heating of thecolumn.

2. A connection system between the inlet valve system and column of agas chromatograph, including,

an oven having a controlled internal temperature,

a thermal insulation body adjacent the oven,

a metallic union mounted on thethermal insulation body and having anaccess opening therethrough from external the insulation body tointernal the insulation body,

a chromatograph column of selected size mounted on the external end ofthe access opening of the union,

a conduit mounted on the internal end of the union and extending throughthe insulation body and into communication with the adjacent oven,

a fluid connection bet-Ween the valve system and conduit which alsoelectrically insulates between the valve system and conduit,

and an electrical power lead extended through the body of insulation toconnect with the column to resistance-heat the column.

, References Cited by the Examiner UNITED STATES PATENTS 259,698 6/82Magin l37575 2,963,898 12/60 Reynolds et al 7323 3,115,766 12/63 Winters7323 OTHER REFERENCES Panchromatogr'aph, a publication of W. G. Pye &Co. Ltd., York Street, Cambridge, England, bulletin No. 150/ 5M/6.62/=F& I, published June 1962.

RICHARD C. QUEISSER, Primary Examiner.

ROBERT L. EVANS, Examiner.

2. A CONNECTION SYSTEM BETWEEN THE INLET VALVE SYSTEM AND COLUMN OF AGAS CHROMATOGRAPH, INCLUDING, AN OVEN HAVING A CONTROLLED INTERNALTEMPERATURE, A THERMAL INSULATION BODY ADJACENT THE OVEN, A METALLICUNION MOUNTED ON THE THERMAL INSULATION BODY AND HAVING AN ACCESSOPENING THERETHROUGH FOR EXTERNAL THE INSULATION BODY TO INTERNAL THEINSULATION BODY, A CHROMATOGRAPH COLUMN OF SELECTED SIZE MOUNTED ON THEEXTERNAL END OF THE ACCESS OPENING OF THE UNION, A CONDUIT MOUNTED ONTHE INTERNAL END OF THE UNION AND EXTENDING THROUGH THE INSULATION BODYAND INTO COMMUNICATION WITH THE ADJACENT OVEN, A FLUID CONNECTIONBETWEEN THE VALVE SYSTEM AND CONDUIT WHICH ALSO ELECTRICALLY INSULATESBETWEEN THE VALVE SYSTEM AND CONDUIT, AND AN ELECTRICAL POWER LEADEXTENDED THROUGH THE BODY OF INSULATION TO CONNECT WITH THE COLUMN TORESISTANCE-HEAT THE COLUMN.